반응 #161895

ord-d2fb62cec9164f48957a19e44449b09d

용매

반응 조건

온도
77°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to cool to room temperature
  2. 2
    추출extracted with 500 ml of ethyl acetate
  3. 3
    기타The organic layer was separated from the solution
  4. 4
    세척washed twice with 100 ml of water and 50 ml of saturated saline
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONAfter distilling off the solvent
  7. 7
    기타the concentrated residue was recrystallized

실험 절차

40.2 g of acrylonitrile was added dropwise to an ethanol solution (150 ml) of 41.7 g of stearylamine at room temperature over 0.5 hours, 22.5 g of acetic acid was added dropwise thereto over 0.5 hours, and then stirred at 77° C. for 10 hours. After standing to cool to room temperature, the mixed solution was added with 200 ml of water and 22.8 g of 28% ammonia water, and extracted with 500 ml of ethyl acetate. The organic layer was separated from the solution, washed twice with 100 ml of water and 50 ml of saturated saline, dried over anhydrous magnesium sulfate. After distilling off the solvent, the concentrated residue was recrystallized using isopropyl alcohol as a solvent to obtain 42.4 g of a target compound as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08830811B2uspto-grants-2014_09